CN104663681A - Abamectin water dispersible nano-composite granule and preparation method thereof - Google Patents
Abamectin water dispersible nano-composite granule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an abamectin water dispersible nano-composite granule and a preparation method thereof. The abamectin nano-granule is prepared from the following raw materials by weight percentage: 30-60% of abamectin loaded on a nano-carrier, 1.0-6.0% of wetting agent, 5.0-10.0% of dispersing agent, 1.0-10.0% of disintegrating agent, 0.1-5% of other accessory ingredients and a filler added to reach 100%. A wet method process is adopted for preparing the abamectin water dispersible nano-composite granule, and a disintegration dispersing type water dispersible granule is prepared through a uniform grain size spray granulation technology. Compared with the traditional dosage form, the abamectin nano-composite granule prepared by the invention has the unique advantages of long-acting slow release, hydrolysis resistance, photolysis resistance, low wastage rate, low toxin, high safety, low using cost and good environment consistency, can be widely applied to many insect pests in the farmland, the orchard and the vegetable field and has an important application value.
Description
Technical field
The invention belongs to biological pesticide technical field, particularly relate to a kind of Avermectin water dispersion nano composite granule and preparation method thereof.
Background technology
Avermectin is the fermentating metabolism product of edaphon streptomyces griseus, the dual-purpose antibiotic of a kind of novel farming animals, special efficacy is had to 10 order 80 various pests such as harmful mite, diamond-back moth, cotton bollworm on the plants such as fruit tree, vegetables, flowers, cotton, tobacco, be widely used in veterinary clinic, be considered to one of biogenic pesticide that preventive effect is best, with fastest developing speed, most widely used in the world at present.Disclosed in existing patented technology, Avermectin is mainly missible oil type, and it is as a conventional dosage forms of agricultural chemicals, control efficiency still can, but there is following problem:
(1) containing organic solvents such as a large amount of toluene, dimethylbenzene, environmental pollution is large;
(2) without controlled-release effect, poor adhesion to target thing, cause the bioavailability of agricultural chemicals low, the term of validity is short;
(3) easily illumination decomposition, facile hydrolysis, cause drug effect to reduce;
(4) need water to be diluted to emulsion when using, effective ingredient belongs to micron order dispersion, and dispersiveness is poor, and effective rate of utilization is low, and cause pesticide dosage large, cause cost to raise, residue of pesticide are large, have a strong impact on the quality of agricultural product.
Water dispersible granules is a kind of pesticides new formulation grown up the eighties in last century, is the product that in current pesticidal preparations, combination property is the most comprehensive and the most perfect, is identified as one of vital formulation of 21 century most.Water dispersible granules agricultural chemicals is made a kind of dry, non-dusting, can free-flow, and a kind of formulations of pesticide easily spread in water.Compared with other formulations of pesticide, water dispersible granules has complied with the development trend of pesticidal preparations Water-borne modification, avoids organic solvents such as using a large amount of toluene, dimethylbenzene, improves Environmental compatibility, to operator's safety, meet the developing direction of energy-saving and emission-reduction.
Nano medicament carrying system is the main application form of nanometer technology in drug delivery, controlled release, it refers to and adopts suitable pharmacy techniques and methods, medicine disperseed, encapsulates, be adsorbed in polymer particle inside or surperficial, make the colloidal drug delivery system of particle diameter in 1 ~ 1000nm scope, mainly contain the citation forms such as nanoparticle, nanosphere, nanocapsule.Compared with conventional dosage forms, nano medicament carrying system has certain slow-release function, can improve drug bioavailability, increases medicine stability, reduces toxic and side effect, and reducing dosage etc., is the very promising drug delivery system of one.In recent years, along with the extensive use of the biopharmaceutical macromolecular drugs such as protein, polypeptide class, immunomodulator and vaccine, drug-carried nanometer system obtains to be paid close attention to widely.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, object is to provide a kind of Avermectin water dispersion nano composite granule and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of Avermectin water dispersion nano composite granule, each components based on weight percentage is: Avermectin 30 ~ 60%, wetting agent 1.0 ~ 6.0%, dispersant 5.0 ~ 10.0%, disintegrant 1.0 ~ 10.0%, and other auxiliary agents 0.1 ~ 5%, filler complements to 100%.
By such scheme, described Avermectin is the Avermectin of load on nano-carrier, and the quality of described Avermectin is 30 ~ 90% of nano-carrier quality.
By such scheme, described nano-carrier is nanoscale imvite, kaolin, goethite, hydroxyapatite or attapulgite.
By such scheme, described wetting agent is one or more in mixture M orwet EFW, the alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425 of alkylnaphthalene sulfonate and anion wetting agent, Sulfonates anion surfactant TERWET1004, lauryl sodium sulfate, neopelex.
By such scheme, described dispersant is one or more in Negel formaldehyde condensation products Morwet D-425, polycarboxylate TERSPERSE2700, alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425.
By such scheme, described disintegrant is one or more in urea, magnesium sulfate, ammonium sulfate, soluble starch.
By such scheme, described filler is one or more in bentonite, kaolin, white carbon.
By such scheme, other auxiliary agents described are adhesive, stabilizing agent, emulsifier or synergist.
The preparation method of above-mentioned Avermectin water dispersion nano composite granule, specifically comprises the steps:
(1) take the Avermectin be carried on nano-carrier, wetting agent, dispersant, disintegrant and filler according to formula, add the water accounting for total quality of material 15 ~ 20% and mixed, obtain water slurry;
(2) above-mentioned water slurry is pumped in grinder grinds, then add a small amount of water and other auxiliary agents, obtain the slip of spraying;
(3) deliver in drying tower by slip, employing waits particle diameter spray granulation to carry out spray drying granulation, after screening, obtain Avermectin water dispersion nano composite granule.
By such scheme, step is ground to ultra-fine wet grinding described in (2), and after grinding, the fineness of slip is 100 ~ 600nm.
By such scheme, described in step (3), the temperature of spray drying granulation is 130 ~ 160 DEG C, and after spray drying granulation, products obtained therefrom residual moisture content is 0.5 ~ 1.0wt%.
By such scheme, screening described in step (3) combines screening for vibrated fluidized bed and vibratory sieve, and after screening, the average grain diameter of described Avermectin water dispersion nano composite granule is 200nm.
The application method of above-mentioned Avermectin water dispersion nano composite granule, is characterized in that: add water Avermectin water dispersion nano composite granule thermoplastic polymer, forms Avermectin suspension and uses.
In the present invention, on nano-carrier, the method for load Avermectin is: Avermectin mixed according to a certain percentage with solvent, makes it dissolve; Porous nano particle is placed in negative-pressure container, repeated multiple times injection abamectin solution, Avermectin is effectively adsorbed in the hole of nano particle; Spray-dried except desolventizing, the Avermectin on nano-carrier must be carried on.
Beneficial effect of the present invention:
(1) the Avermectin water dispersion nano composite granule that prepared by the present invention has and significantly controls slow-release function, effectively can extend the lasting period of Avermectin under same dose, improve the availability of agricultural chemicals, reduce dosage, thus reduction pesticide cost and agricultural chemicals are to the pollution of environment;
(2) particle diameter of Avermectin water dispersion nano composite granule prepared of the present invention is little, and surface tension is low, has fabulous permeability, wetability, levelability and rheological characteristic, directly can infiltrate in the fine duct of plant, make agricultural chemicals high degree of dispersion; Also there is hydrolysis, resistance to photodissociation, good stability, advantage that turnover rate is low simultaneously;
(3) the Avermectin water dispersion nano composite granule prepared of the present invention, adopts the dosage form design of Water-borne modification, avoids the use of organic solvent, decrease the discharge of toxic organic solvents, gives the compatibility that environment is higher;
(4) the particle diameter prilling such as preparation method's employing of the present invention, optimizes the microstructure of Avermectin water dispersion nano composite granule, makes it more can meet the requirement of moment disintegration in water, has significant technical advantage.
Embodiment
In order to understand the present invention better and embody outstanding advantage of the present invention, especially exemplified by going out following embodiment, special needs to be pointed out is following examples just example, can not as the restriction of applying the present invention.
In following examples, method Avermectin be carried on nano-carrier is: Avermectin mixed with the ratio of ethylene glycol according to mass ratio 1:2 ~ 5, after Avermectin is dissolved completely, porous nano particle is placed in negative-pressure container, repeated multiple times injection abamectin solution, makes Avermectin effectively be adsorbed in the hole of nano particle; Spray-dried removing ethylene glycol, must be carried on the Avermectin on nano-carrier.Show after testing, the pay(useful) load rate (Avermectin accounts for the percentage by weight of nano-carrier) of Avermectin is 30 ~ 90%.
Embodiment 1
Avermectin water dispersion nano composite granule, prepare by the following method: accurately take the Avermectin 30.0kg be carried on nano imvite according to recipe requirements, wetting agent is the Morwet EFW of 1.0kg, dispersant is the Morwet D-425 of 10.0kg, disintegrant is the urea of 1.0kg, filler is the white carbon of 57.9kg, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the synergist of certain water gaging and 0.1kg, obtain the slurry of spraying, again slip is delivered to drying tower, spray drying granulation at 130 DEG C, after granulation, product residual moisture content is 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm.
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, be that 400mg/L is (with Avermectin content meter at drug concentration, lower same), after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.11 ± 1.34%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 86.12 ± 2.13 and 96.88 ± 3.21%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
Embodiment 2
Avermectin water dispersion nano composite granule, prepare by the following method: accurately take the Avermectin 35.0kg be carried on nano kaoline according to recipe requirements, wetting agent is the lauryl sodium sulfate of 2.0kg, dispersant is the polycarboxylic acid salt TERSPERSE2700 of 5.0kg, disintegrant is the magnesium sulfate of 2.0kg, the ammonium sulfate of 3.0kg, filler is the bentonite of 30.0kg, the kaolin of 20kg, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the adhesive of certain water gaging and 3.0kg, obtain the slurry of spraying, again slip is delivered to drying tower, spray drying granulation at 140 DEG C, after granulation, product residual moisture content is 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm.
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, at drug concentration 400mg/L, after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.33 ± 2.31%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 86.31 ± 3.16 and 97.81 ± 2.45%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
Embodiment 3
Avermectin water dispersion nano composite granule, prepare by the following method: accurately take the Avermectin 40.0kg be carried on nanoneedle iron ore according to recipe requirements, wetting agent is the TERSPERSE2425 of 3.0kg, the neopelex of 3.0kg, dispersant is 3.0kg polycarboxylate TERSPERSE2700, 4.0kg alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425, disintegrant is magnesium sulfate 5.0kg, soluble starch 5.0kg, filler is the bentonite of 18.3kg, 13.7kg white carbon, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the stabilizing agent of a small amount of water and 5.0kg, obtain the slurry of spraying, again slurry is delivered to drying tower, spray drying granulation at 150 DEG C, after granulation, product residual moisture content is 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm.
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, at drug concentration 400mg/L, after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.81 ± 2.44%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 85.72 ± 4.11 and 97.23 ± 3.02%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
Embodiment 4
Avermectin water dispersion nano composite granule, prepare by the following method: the Avermectin accurately taking the 48.5kg be carried on nanometer hydroxyapatite according to recipe requirements, wetting agent is the Sulfonates anion surfactant TERWET1004 of 2.2kg, the neopelex of 3.8kg, dispersant is 3.0kg polycarboxylate TERSPERSE2700, the alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425 of 4.0kg, disintegrant is the magnesium sulfate of 2.0kg, the ammonium sulfate of 3.5kg, filler is the bentonite of 31.5kg, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the adhesive of certain water gaging and 1.5kg, obtain the slurry of spraying, again slurry is delivered to drying tower, spray drying granulation at 130 DEG C, after granulation, product residual moisture content is 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm.
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, at drug concentration 400mg/L, after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.66 ± 5.32%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 86.52 ± 2.43 and 96.91 ± 3.52%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
Embodiment 5
Avermectin water dispersion nano composite granule, prepare by the following method: accurately take the Avermectin 50.0kg be carried on nano-attapulgite according to recipe requirements, wetting agent is the Sulfonates anion surfactant TERWET1004 of 3.3kg, the lauryl sodium sulfate of 2.7kg, dispersant is the alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425 of 7.8kg, disintegrant is the magnesium sulfate of 2.0kg, the ammonium sulfate of 3.5kg, filler is the bentonite of 29.0kg, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the stabilizing agent of certain water gaging and 1.7kg, obtain the slurry of spraying, again slurry is delivered to drying tower, spray drying granulation at 140 DEG C, after granulation, product residual moisture content is at 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, at drug concentration 400mg/L, after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.41 ± 1.54%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 86.93 ± 2.73 and 96.18 ± 3.92%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
Embodiment 6
Avermectin water dispersion nano composite granule, prepare by the following method: accurately take the Avermectin 60.0kg be carried on attapulgite according to recipe requirements, wetting agent is the Sulfonates anion surfactant TERWET1004 of 2.3kg, the lauryl sodium sulfate of 1.7kg, dispersant is the alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425 of 2.5kg, the Negel formaldehyde condensation products Morwet D-425 of 2.7kg, disintegrant is the magnesium sulfate of 2.6kg, the ammonium sulfate of 3.5kg, filler is 10.0kg bentonite, 10.0kg kaolin, the water adding 15 ~ 20kg is mixed, obtain suspension, being ground to fineness with ultra-fine wet grinding mill is again 100 ~ 600nm, add the stabilizing agent of certain water gaging and 4.7kg, obtain the slurry of spraying, again slurry is delivered to drying tower, spray drying granulation at 160 DEG C, after granulation, product residual moisture content is 0.5 ~ 1.0wt%, finally material vibrated fluidized bed and vibratory sieve are combined screening, obtain the Avermectin water dispersion nano composite granule that average grain diameter is 200nm.
The quality index of the Avermectin water dispersion nano composite granule that the present embodiment prepares is in table 1, to javanese root knot nematode second instar larvae active testing, at drug concentration 400mg/L, after process 24h, Avermectin water dispersion nano composite granule process nematode corrected mortality is 85.67 ± 6.32%, and conventional Avermectin process lethality is only 71.12 ± 2.12%.When drug concentration is 100mg/L and 200mg/L, after chemicals treatment 48h, the nematode corrected mortality of Avermectin water dispersion nano composite granule process is respectively 86.79 ± 6.14 and 96.16 ± 3.52%, and the nematode corrected mortality of Avermectin conventional formulation process is 53.12 ± 2.12% and 61.41 ± 4.36%.
As can be seen from the above embodiments, Avermectin water dispersion nano composite granule prepared by the present invention to javanese root knot nematode second instar larvae to kill line active in Avermectin conventional formulation, what after the processing time extends, Avermectin water dispersion nano composite granule can reach Avermectin conventional formulation higher concentration kills line level, reflects Avermectin water dispersion nano composite granule prepared by the present invention and has slowly-releasing, efficiently characteristic.
Table 1 Avermectin water dispersion nano composite granule quality index
Above-described embodiment shows, Rynaxypyr water dispersion nano composite granule of the present invention is obvious to various pests control efficiency, and has slow release effect, and duration of efficacy is long.And this water dispersible granules take water as medium, environmental protection, intragranular disintegration speed is fast, there is no bales stained, not easily key is produced to environment, people and animals and other biological, and insect not easily develops immunity to drugs to it, and reduce Pesticide use amount, reduce the production cost of product.In addition, the cold and hot bin stability of water dispersible granules of the present invention is good, and technique is comparatively simple, and suitability for industrialized is produced and large scale application.
Claims (10)
1. an Avermectin water dispersion nano composite granule, is characterized in that, each components based on weight percentage is:
Avermectin 30 ~ 60%, wetting agent 1.0 ~ 6.0%, dispersant 5.0 ~ 10.0%, disintegrant 1.0 ~ 10.0%, other auxiliary agents 0.1 ~ 5%, filler complements to 100%.
2. Avermectin water dispersion nano composite granule according to claim 1, is characterized in that, described Avermectin is the Avermectin of load on nano-carrier, and the quality of described Avermectin is 30 ~ 90% of nano-carrier quality.
3. Avermectin water dispersion nano composite granule according to claim 2, is characterized in that, described nano-carrier is nanoscale imvite, kaolin, goethite, hydroxyapatite or attapulgite.
4. Avermectin water dispersion nano composite granule according to claim 1, it is characterized in that, described wetting agent is one or more in mixture M orwet EFW, the alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425 of alkylnaphthalene sulfonate and anion wetting agent, Sulfonates anion surfactant TERWET1004, lauryl sodium sulfate, neopelex.
5. Avermectin water dispersion nano composite granule according to claim 1, it is characterized in that, described dispersant is one or more in Negel formaldehyde condensation products Morwet D-425, polycarboxylate TERSPERSE2700, alkyl naphthalene sulfonic acid condensation polymer TERSPERSE2425.
6. Avermectin water dispersion nano composite granule according to claim 1, is characterized in that, described disintegrant is one or more in urea, magnesium sulfate, ammonium sulfate, soluble starch.
7. Avermectin water dispersion nano composite granule according to claim 1, is characterized in that, described filler is one or more in bentonite, kaolin, white carbon.
8. Avermectin water dispersion nano composite granule according to claim 1, is characterized in that, other auxiliary agents described are adhesive, stabilizing agent, emulsifier or synergist.
9. the arbitrary described Avermectin water dispersion nano composite granule of claim 1 ~ 8 preparation method, it is characterized in that, comprise the steps:
(1) take the Avermectin of load on nano-carrier, wetting agent, dispersant, disintegrant and filler according to formula, add the water accounting for total quality of material 15 ~ 20% and mixed, obtain water slurry;
(2) be pumped in grinder by above-mentioned water slurry and grind, after grinding, the fineness of slip is 100 ~ 600nm, then adds a small amount of water and other auxiliary agents, obtains the slip of spraying;
(3) deliver in drying tower by slip, employing waits particle diameter spray granulation to carry out spray drying granulation, and the temperature of spray drying granulation is 130 ~ 160 DEG C, then obtains the Avermectin water dispersion nano composite granule that average grain diameter is 200nm after screening.
10. the application method of the arbitrary described Avermectin water dispersion nano composite granule of claim 1 ~ 8, is characterized in that: be added to the water Avermectin water dispersion nano composite granule thermoplastic polymer, forms Avermectin suspension and uses.
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Application publication date: 20150603 |